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Article history: A type IV composite pressure vessel subjected to fire may burst because of the degradation
Received 11 April 2017 of the outer layers, but when the inner pressure is less than a critical value, leak is observed
Received in revised form instead of burst. This phenomenon is due to the heat transfer through the composite shell
8 June 2017 which leads to liner melting. In order to characterize this failure mechanisms, engulfing
Accepted 11 June 2017 fire tests have been performed in the framework of the FireComp project whose objective is
Available online xxx to understand and simulate the fire performance of hydrogen storage. An experimental
set-up has been implemented to expose the cylinders to fire by the means of gas injectors.
Keywords: A simple FE model has been developed to simulate the coupled effects of mechanical
Wound composite vessel damage and of temperature. This approach is found to accurately predict the time to burst
Hyperbaric hydrogen tank of the composite tank, as well as the transition between burst and leak.
Fire tests © 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
Thermomechanical behavior
Burst simulation
Leak
* Corresponding author.
E-mail address: damien.halm@ensma.fr (D. Halm).
http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
0360-3199/© 2017 Hydrogen Energy Publications LLC. Published by Elsevier Ltd. All rights reserved.
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
2 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
European R&D collaborative project management (Ayming). material characteristics (moduli, strength …). In spite of this
The main objective of the FireComp project is thus to better highly coupled framework, the numerical tools have to be
characterize the conditions that are required to prevent the simple enough to simulate large vessels, but they must also
tanks from bursting. To this aim, experimental work is carried provide a high level of reliability. In this study, a basic, simple
out, in a first step, to improve understanding of the heat criterion approach has been considered, in which the com-
transfer mechanisms and the loss of strength of composite posite ply fails as soon as a damage criterion is satisfied. In
high-pressure vessels in fire conditions. In a second step, Ref. [13], usual criteria (maximum stress, Hoffman, Tsai-Hill
tractable and reliable simulations of the thermo-mechanical and Tsai-Wu) are compared to simulate the burst pressure
behavior of the high pressure vessel exposed in the same of a composite hydrogen storage vessel subjected to inner
conditions are necessary. They will allow, in the future, to pressure. It is proven that these criteria lead to very similar
improve current standards and fire protection strategies in burst pressure predictions: all of them forecast a burst pres-
order to protect people from both cylinder burst and hydrogen sure with a maximum deviation of 5% compared to the
flames. Even if burst in service of pressure vessels in com- experimental test. A similar conclusion is drawn in Ref. [14]
posite material is very unlikely, when exposed to a fire, a which compares more complex damage models: the
typical compressed hydrogen tank presents safety challenges simplest approaches (e.g. progressive failure analysis) provide
and protection means need to be sized to avoid burst and limit sufficiently reliable prediction of the burst pressure. Conse-
hazardous effects of hydrogen release. quently, for the sake of tractability, a maximum stress failure
The risk for fire and thereby degradation of the composite criterion is selected in this work: failure in a ply is assumed to
material in fire must be better understood, so that the right occur when the stress in the fiber direction reaches the cor-
measures are taken to mitigate risks associated with the use responding temperature-dependent strength. Due to the ten-
of composite cylinders. According to the type of application sion stress state in the pressurized composite tank it is not
(gas transportation, on-board vehicle hydrogen storage, …) necessary to add criteria in compression.
different tank sizes may enter the market, which would have The abundant literature [15e21] that deals with the burst
very different impact in terms of consequences in case of strength determination of wound storage subjected to internal
burst or in case of hydrogen release, but also a very different pressure (by the means of analytical models or of FE simula-
behavior in fire, mainly due to different thickness and inner tions), at room or moderate (80 C) temperature, proves the
pressure. This is also why it is necessary to develop models current interest of the subject. Unlike the case of metallic ves-
that allow predicting the behavior of large and thick cylinders sels, burst of composite tanks subjected to fire is not due to
that cannot be tested due to safety and cost constraints. The pressure increase: when the matrix of the outer layers directly
behavior of thick composite structures in fire is therefore the exposed to fire is degraded, the composite transforms into char,
main topic to model and validate, as input to the standardi- a material whose mechanical properties are strongly reduced
zation and regulatory bodies. [22]. This chemical reaction, which can be mechanically
The risk analysis [5] and the prediction of storage burst considered as a type of damage, substantially modifies the
capability in fire are subjects of great current interest. This stress distribution within the structure: the stress undergone by
topic has been addressed by Zheng et al. [6,7] through CFD the outer burnt layers is transferred to the inner layers which
simulation of bonfire tests in order to investigate the effects of rapidly reach their damage threshold and the global strength is
fuel type, fuel flow and filling medium on internal tempera- strongly reduced. As the thickness of the actual storage struc-
ture rise of pressure vessels subjected to engulfing or localized tures prevents from direct testing on conventional mechanical
fire. In these latter works, loss of load-bearing capacity of the test machines, the coupled mechanical/thermal/decomposi-
wound composite shell is not taken into account. Hu et al. [8] tion model has to be identified from representative samples cut
coupled thermal simulations and mechanical damage in a in wound tubes. The experimental data presented in Refs.
Finite Element model and predicted the profile of resin con- [23e26] have been used for model identification and validation.
tent in the hydrogen storage vessel but the results of the Another difficulty has to be explicitly overcome: whereas
simulations are not explicitly compared to experimental time the simulation of the thermomechanical behavior at the
to burst of pressurized vessels subjected to fire. In order to sample scale has been already addressed in Ref. [24], the
assess the duration a pressurized vessel can withstand fire present paper has to tackle the challenging FE simulation of
without burst, the first step is the determination of the ther- real type IV pressurized vessels subjected to fire, that means
mal and mechanical properties of the wound composite ma- structures containing a priori a very large number of degrees of
terial the tank is made of, and the choice of the more freedom. Consequently, geometrical assumptions (e.g.
convenient approach to model the composite degradation. axisymmetry) or simple ways to take into account thermo-
Mechanical damage models at different scales can be found in mechanical couplings are implemented to reduce the com-
the literature [9e11] to forecast the progressive degradation of puter time. The comparison of the simulation results with fire
composites. The study presented in these pages adds a sup- tests are used to validate the modelling approach and to
plementary difficulty, namely coupling between mechanical identify its limits. Indeed, the partner INERIS has carried out a
loading, temperature and fire. The simulation of the tank large set of fire experiments on different types of tanks (19 L,
behavior cannot be carried out without a reliable thermo- 36 L), filled with different gases (nitrogen, hydrogen, helium)
mechanical behavior model. Indeed, the temperature at different inner pressure (100 bar, 250 bar, 525 bar, 700 bar).
gradient leads to an important modification of the stress dis- For that purpose, a specific experimental set-up involving four
tribution within the composite structure. Moreover, tests [12] hydrogen injectors and a confinement, made of concrete
have shown a significant influence of temperature on the panels, has been designed. It allows to ensure a quite
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 3
homogeneous distribution of heat flux around the vessel and a properties are well known. The external dimensions of the
level of energy in accordance with conventional bonfire pool steel cylinder are the same as those of the 36-L composite
tests. These thermomechanical tests have been instrumented cylinders that will be used in the next phase, as shown in
by inserting thermocouples in the vessel composite wall at Fig. 1. The sealing of the cylinders is ensured by copper seals,
different depths and different locations. The pressure inside to enable pressure measurements. The weight of the cylinder
the vessel was also measured during all the tests. Details is about 196 kg.
about these tests are given in Section Fire tests on pressure In addition to the pressure measurement, the evolution of
vessels. temperature is recorded by 24 thermocouples marked by red
In order to check the validity of the FE simulations, a given points in Fig. 1:
tank geometry of 36 L has been selected as a reference case.
The geometry of the liner and of the metallic bosses, as well as 8 on the internal face of the cylinder,
the exact composite lay-up (orientation and thickness of each 8 on the external face of the cylinder,
layer), has been provided by the partner Hexagon (but not 8 in the flame region.
disclosed in this article, for the sake of confidentiality).
Coupled thermomechanical calculations are performed to In order to increase the amount of energy that can be
reproduce the experimental conditions undergone by the transmitted to the cylinder during gas fires and improve the
vessel: the tank is subjected to a constant inner pressure of homogeneity of the thermal aggression around it, a confine-
700 bar and an incident heat flux representative of the thermal ment is placed above the set-up. The material used to make
aggression of the four hydrogen injectors. Two experimental this confinement is standard aerated concrete. A picture of the
data are compared to the results of the simulations: the time experimental setup is displayed in Fig. 2.
to burst (or to leak, depending on the inner pressure) and the Since the tests can be done with cylinders of various di-
temperature measured by thermocouples placed in the com- mensions (19 L, 36 L), the geometrical definition of the
posite wall. confinement is done relatively to the external walls of the
In a first part, the experimental setup allowing subjection cylinder, as presented in Fig. 2. This approach allows defining
of a pressure vessel to a fire, which is representative of an completely the confinement regardless of the size of the
accidental condition and the main results are described. The tested cylinder.
geometry of the corresponding simulated vessel is then As mentioned previously, the cylinder is exposed to fire by
detailed in the second part, and the materials' characteristics the means of four injectors. They are symmetrically located
are recalled. The emphasis is then directed to the input data under the cylinder as presented in Fig. 2. This position pro-
and the way to model as simply as possible the thermo- vides a satisfactory engulfment of the cylinder. On each
mechanical couplings. At last the results at different inner injector, a calibrated flow rate of hydrogen and oxygen
pressures are presented and discussed. mixture can be controlled.
This setup differs from usual bonfire tests [27,28]. In gen-
eral, these tests are performed by the means of a heptane
Fire tests on pressure vessels pool, whose liquid level is regulated by injection in order to
reach a constant flame regime. The drawbacks of this type of
Full-scale fire experiments have been carried out on pressure bonfire test are a large quantity of heptane mist leading to
vessels by the partner INERIS. They comprise of two steps. The secondary explosions, after cylinder burst, and the necessity
first step aims at determining the fire conditions to test the to extract fumes to allow visibility.
thermo-mechanical behavior of composite vessels in real By contrast, hydrogen gas fires have significant advan-
conditions. Those conditions have to be representative of tages. Firstly, hydrogen gas fire is the more realistic scenario
accidental situations and represent worst case scenarios when assessing safety of these pressure vessels since
regarding the suspected fire vulnerability of the reservoir. hydrogen is the combustible whose presence is the most likely
They also need to be operated (instrumented) in order to near hydrogen storage. Secondly, it is important to note that
determine the incident equivalent heat flux and to record gas fires are not too complex to calibrate and not too expen-
valuable experimental data to be compared to the modelling sive experimentally, whereas standard pool bonfires involve
results. These preliminary tests were performed using a steel repeatability issues due to ventilation, soot deposit and high
cylinder. impact of the vessel size on the flame.
The second part of the study is performed on real com- The hydrogen gas fire tests are carried out with 1.5 g/s
posite vessels, using the thermal aggression determined in the hydrogen and 0.5 g/s oxygen flow rates per injector. In order to
first step. impose realistic values in numerical simulations, it is neces-
sary to measure the mean incident flux absorbed by the cyl-
Determination of experimental setup and fire conditions inder when subjected to fire. A simple reasoning, together
with some assumptions, allows to have access to an estima-
These preliminary tests were performed using a steel cylinder tion of this flux noted fcyl in the following. The experimental
(whose size is similar to the composite cylinder) in order to input is the evolution of the temperature inside the vessel. It
calibrate the heat load measurement method and study the can be determined by measuring the gas pressure in the cyl-
reproducibility of the fire. Thanks the use of metallic vessels in inder and by assuming air is an ideal gas. As the cylinder be-
this preliminary study, there are no issues related to the haves as a calorimeter, it is possible to calculate the heat flux
thermal decomposition of the specimen and the thermal fSi/g transmitted by the internal surface Si by differentiating
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
4 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 5
the thermal energy Eg stored by the gas (air) in the cylinder by the partner Hexagon [30] and are obtained by filament
when temperature increases (this energy can be calculated composite winding [31] on a polymer (High Density Poly-
from the measured temperature of the gas Tg, the mass of gas ethylene) liner and a metallic (aluminum alloy) boss, one at
mg and its specific heat capacity Cg): each end. The boss allows connecting the tank to the fuel cell,
the liner ensures the tightness of the vessel whereas the role of
dEg
fSi /g ,Si ¼ (1) the composite shell is to withstand the inner pressure. The in-
dt
service pressure is 700 bar. During manufacturing, thermo-
with Eg ¼ mg ,Cg ,DTg , DTg being the temperature rise. Once couples have been inserted in the composite wall, at different
fSi/g is known from the previous equation, it is possible to depths and different locations. The position and the number of
estimate the average temperature TSi of the internal surface of each thermocouple are detailed in Fig. 4. The pressure inside
the cylinder, provided the areal transfer coefficient h does not the vessel is also measured during the tests.
vary significantly during the test. This coefficient can be Among more than 30 tests carried out on different cylin-
estimated at about 4.4 W/m2 K [29]. ders to analyze the influence of specimen size, filling media,
duration of thermal exposure, initial pressure …, the tests
fSi /g ¼ h, TSi Tg (2)
selected here provide information about repeatability and
The estimation of the net heat flux fcyl absorbed by the cyl- initial pressure influence. Note that the effect of the fill gas has
inder requires the temperature at the outer surface. Given the been studied in a preliminary step by comparing the time to
high thermal conductivity of the steel the cylinder is made of burst or leak when the pressurizing gas is helium, nitrogen or
and the small thickness of the wall, the temperature gradient hydrogen. Since no significant difference has been observed,
through the steel wall DT is small. It can be estimated by the all tests presented in the following have been carried out with
means of the relation by fcyl ¼ lsteel DT, where lsteel ¼ 35 W/m K is nitrogen, for reasons of safety and cost.
e
The experimental setup is described in the previous sec-
the steel thermal conductivity (in the measured temperature
tion and is illustrated in Fig. 4. Fig. 5 presents the evolution of
range) and e ¼ 25 mm the cylinder wall thickness. As it will be
internal pressure of two repeatability tests (number 21 and
shown in the following, the heat flux fcyl ranges between 80 kW/
22), performed on 36-L cylinders.
m2 and 100 kW/m2. As a consequence, the temperature gradient
First of all, these curves confirm a well-known result
is approximately 65 C which is low compared to the tempera-
regarding the failure mode of composite cylinders. Unlike
ture of the internal surface (~650 C). It is then acceptable to
steel cylinders, burst does not occur because of the pressure
consider that the temperature is constant in the thickness of
increase which is very low in that case, but because of
the cylinder wall, and is equal to the internal surface.
degradation of mechanical properties.
Since the temperature at the internal surface is close to the
During the first 100 s, the internal pressure undergoes a
temperature at the outer surface, the net heat flux fcyl absor-
slight decrease of 2.5 bar, and afterwards an increase until
bed by the vessel can be calculated thanks to the evolution of
burst. This phenomenon can be explained by the fact that
TSi, the cylinder mass mcyl, its external surface Sext and its
vessels were filled just before the test, and stabilization of
specific heat capacity CPsteel (300 J/kg.K at the considered
pressure and temperature was not fully achieved. Fig. 5 high-
temperature range):
lights repeatability of the thermal aggression of the cylinders:
dTSi in both cases, burst occurs after nearly 240 s and a pressure
fcyl ,Sext ¼ mcyl ,CPsteel , (3)
dt increase of 15 bar. Burst is detected by the sharp pressure drop.
Fig. 6 plots the evolution of wall temperature at different
This net heat flux is a lower bound to the total incident heat points for reference test 21 (T10, T11 and T12 are respectively
flux which also takes into account the radiative heat flux the thermocouples recording temperature of the outer layers,
emitted by the cylinder. According to the aforementioned pro- of the middle of the wall and of the inner layers close to the
cedure to determine fcyl, the evolution of the net heat flux liner). Just before bursting, the temperature near the liner is
received by the cylinder is plotted in Fig. 3a. The value of this flux about 95 C, while it has reached 400 C on the external layer of
fluctuates over test time around a mean level. An approximation the cylinder. This figure also illustrates the delay of propaga-
of the average value of 90 kW/m2 can be retained, considering tion of heat along the composite wall, which will be useful
that after 400 s, the temperature rise of the cylinder increases the information regarding modelling.
radiative heat flux emitted by the external surface. As mentioned previously, one of the parameters studied in
Fig. 3b displays the evolution of the temperature recorded this work is the initial inner pressure. Fig. 7 plots the pressure
by the external thermocouples at 50 mm of the vessel. It can evolution over test time for different initial values. These tests
be observed that the temperature predominantly fluctuates have been useful to define a depressurization strategy, which
between 800 C and 1000 C. This dispersion is of the same allows keeping the cylinder with an internal pressure that
amplitude as the one measured during bonfire tests with a does not lead to burst. For the tests 21 (initial pressure 700 bar)
heptane pool [28]. This highlights the reliability of the non- and 24 (initial pressure 525 bar), burst occurs after 238 s and
standard hydrogen gas fire tests. 311 s respectively. However, no burst is observed for the tests
25 and 26. The progressive pressure decrease (after 400 s and
Experimental time to burst/leak 490 s respectively) is an evidence for vessel leak. This transi-
tion burst/leak may be useful to define a pressure relief
The internal volume of the reference type IV wound composite strategy avoiding burst on the one hand and total gas
cylinders studied in this work is 36 L. They are manufactured emptying on the other hand.
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
6 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
Fig. 3 e Results of the calibration tests: a. net heat flux absorbed by the vessel, b. temperatures at 50 mm of the cylinder.
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 7
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
8 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
Fig. 6 e Evolution of wall temperature e Reference and repeatability tests (the position of the thermocouples is recalled in
the figures).
regarding the vessel geometry, the composite material for each layer, the winding angle (measured with respect to the
behavior and the boundary conditions are presented. tank axis) and the thickness. Owing to confidentiality of the
industrial process, the exact lay-up is not disclosed in this
Geometry and composite shell paper. Fig. 8 shows a representation of the lay-up: each color
stands for a given angle. Note that because of the winding
The reference 36-L tank whose thermomechanical behavior process, each layer is composed of two interlaced “sub-layers”
has been experimentally studied in the previous part is (þq and -q, where q is the layer angle). The mechanical behavior
modelled by Finite Element Analysis (software Abaqus). A of each sub-layer is considered as transversely isotropic.
picture of this 36-L tank is displayed in Fig. 8. It is recalled that Whereas the thickness and the angle of the layers remain
the type IV pressure vessels are obtained by filament winding constant in the cylinder, it is well known [31] that these
process over a polymeric liner and metallic bosses at the ends. geometrical parameters evolve in the dome. For example, the
Beside the geometry of the bosses and of the liner, the FE angle of the tow increases up to 90 near the pole, then the
computations require the full stacking sequence of the wound composite filament turns around the pole and goes back to-
composite shell in the cylindrical part of the vessel, that means, wards the cylindrical part. Different theories account for these
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 9
Fig. 8 e 36-L tank, representation of the composite lay-up (the grey layer at the bottom is the liner) and axisymmetric FE
geometry.
evolutions [32]. In the context of the project FireComp, a From these experiments, it is possible to identify the in-
simple, pragmatic approach has been chosen: the lay-up plane elastic moduli and the material strength, for each
(thickness and angle of each layer) is assumed to be iden- temperature. These elastic mechanical properties and
tical in the cylinder and in the dome. This approach is called strength values are completed by data coming from the fiber
“constant lay-up” in the following. Although this hypothesis is supplier [33] and from literature [34] (in particular the prop-
quite strong, it is assumed that the cylinder bursts in the erties in the fiber direction). The following conclusions
centre section and that the design of composite at the dome regarding the mechanical properties can be drawn:
has no major influence on the burst pressure. As the explosion
totally destroys the cylinder, it is not possible to observe a The longitudinal modulus (130 GPa at 20 C) is only slightly
posteriori the position of burst initiation. affected (decrease of 15%) by the temperature in the range
20 Ce150 C, whereas the transverse stiffness (4.8 GPa at
Materials' characteristics and geometrical assumptions 20 C) and the in-plane shear modulus (9.2 GPa at 20 C)
drop by a factor of around 10 once the glass transition
The composite material used to manufacture the pressure temperature is reached. The evolutions of the relative
vessels is composed of an epoxy resin (whose glass transition stiffness (which is defined as the ratio stiffness at current
temperature is about 108 C) and T700S carbon fibers [33], with temperature/stiffness at room temperature) in the range
a volume fiber ratio of about 55%. An extensive test campaign [20 C-150 C] determined from the aforementioned tests
on composite samples cut in real pressure vessels (in order to and data are plotted in Fig. 9 and are found to be consistent
be representative of the actual wound composite material) with work dealing with similar materials [8,35,36].
has been carried out in the framework of the FireComp proj- The longitudinal strength, noted X in the following, remains
ect. This campaign is composed of: identical (2.5 GPa), whatever the temperature (as long as
pyrolysis does not occur), the transverse strength (noted Y,
Tension tests up to fracture [23,24] at room temperature, at 15 MPa at 20 C) is strongly reduced above 108 C (the ma-
50 C, at 80 C and at 150 C performed on parallelepipedic terial loses more than 90% of its strength in this direction) as
samples. Since the diameter of the cylinder in which the well as the shear strength (noted S, 62 MPa at 20 C).
samples are cut is 1 m, the coupons are almost flat. The
dimensions of the samples are: 300 mm 25 mm 5 mm. Regarding the thermal properties, an inverse modelling
Four different stacking sequences are tested: ±12 , ±45 , 90 approach based on a constant thermal conductivity and a
and a quasi-isotropic sequence (±12 /90 /±45 /90 ). For each temperature dependent heat capacity is used [25,26]. The
test, the applied axial force vs. axial strain curve is recorded. hypothesis of a constant thermal conductivity is proposed so
Cone calorimeter experiments on thicker (29 mm) samples as to reduce the degrees of freedom in the inverse modelling
[25,26] were performed to capture the thermal behavior of and to avoid inconsistent trends between the model and the
the material (thermal properties and charring rate). Ther- experimental results. The conductivity of the composite is
mocouples were inserted at different thicknesses and equal to 0.48 W/m K in the directions normal to the layers and
recorded the evolution of the temperature during the test normal to the fibers whatever the temperature. The conduc-
(exposure to a controlled incident flux). Experiments were tivity in the fiber direction is taken ten times greater than this
run at external incident heat flux of 30 kW/m2. Three to value, according to Hu et al. [8]. The heat capacity follows a
four repetitions were performed in order to assess the 0:76
consistency of the obtained results. power law: Cpcomp ¼ 389 20 T
(in J/kg.K, T is the temperature
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
10 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
Fig. 9 e Evolution of the longitudinal, transverse and shear relative moduli vs. temperature.
in C). These tests also allow identification of the temperature (combustion stop), the stiffness is less than 10% of its initial
at combustion onset of the composite (~350 C) and at com- value. Between 350 C and 450 C, the material density
bustion stop (~450 C). The radiative transfer at the composite decreases from 1350 kg/m3 to 1015 kg/m3. Regarding the
surface when charring takes place has been measured by the transverse and shear moduli, their values, very low at
partner LEMTA [37]. It is concluded the emissivity has to be set 150 C, do not need to be further affected. Note that this
to 0.91. direct temperature dependence of stiffness prevents from
The liner is High Density PolyEthylene (HDPE), whose simulating mechanical residual strength after cooling
behavior is assumed to be elastic, given its negligible contri- down (stiffness would return to its initial value). This is not
bution to the global stiffness. Its Young's modulus is a drawback since simulations are carried out up to failure.
900 MPa at room temperature, its Poisson's ratio 0.4. The As already stated, the effect of temperature and of com-
bosses are made of 6061 aluminum alloy, whose Young's bustion on the thermal properties of the composite mate-
modulus is 69 GPa and Poisson's ratio 0.3. As for the HDPE, the rial is taken into account through the evolution of the heat
6061 alloy is assumed to behave elastically. This hypothesis is capacity Cpcomp, while the conductivity is assumed to
acceptable for the coupled loading case (incident flux þ inner remain constant [25].
pressure) since the stress state due to the pressure of 700 bar is
far below the elastic yield of the metal. The evolution of the longitudinal, transverse and shear
Multiphysics couplings are a major difficulty of the struc- moduli from room temperature to the end of combustion
tural computation presented in this study. In order to avoid (450 C) is schematically synthesized in Fig. 9.
prohibitive computer times, a simplified strategy is based on The burst simulations take advantage of the symmetries of
the following relationships between temperature, mechanics the problem: the geometry is axisymmetric (only a slice of the
and combustion: vessel is represented) and only one half of the tank is modelled
(Fig. 8). This geometry is meshed with axisymmetric quadratic
The mechanical elastic stress is assumed to have no in- elements. Thanks to this geometrical assumption, the number
fluence on the material combustion and on the thermal of elements is limited and the computation time reduced (6851
properties elements for the boss and the liner, 15713 for the composite;
As already mentioned, the mechanical stiffness is affected by the thickness of each composite layer contains one element).
the temperature. Its evolution over the interval 20 C-150 C
has been addressed above. Between 150 C and the com- Loading and boundary conditions
bustion start temperature (350 C), the stiffness is supposed
to remain constant, since the TGA experiments [23] do not The applied loading and boundary conditions are in accor-
exhibit specific chemical reactions in this temperature range. dance with the tests performed by INERIS and presented in
The temperature controls combustion, but instead of Section Fire tests on pressure vessels:
integrating coupled Arrhenius laws (see f. ex. [38]) to model
the transformation of the composite into char, combustion Symmetry conditions are applied along the mirror plane
is implicitly taken into account by its effect on the me- (on the right-hand side of the geometry in Fig. 8). The
chanical stiffness. Starting from the experimental obser- metallic boss is free to move along its axis, allowing the
vation showing the char has no residual strength [23], it is elongation of the cylinder.
assumed that the longitudinal modulus sharply drops from A pressure is applied on the inner surface of the liner and
the combustion onset temperature (350 C). At 450 C the boss. The value of the pressure is 700 bar, which is the
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 11
in-service working pressure and the reference pressure of 700 bar and an incident flux of 100 kW/m2 and to compare the
the fire tests. results to the experiments presented in Section 2. It is recalled
The incident flux measurement detailed in Section 2 leads that the 36-L vessels subjected to fire have been instrumented
to a value fluctuating between 80 kW/m2 and 100 kW/m2. by thermocouples placed close to the outer surface (top), in
Since this measure represents the net flux (measured from the middle of the composite shell (middle) and close to the
the temperature increase in the cylinder, see Section 2.1), it interface liner e composite (bottom). Fig. 4 shows the location
is chosen to prescribe the upper bound (100 kW/m2) of this of these thermocouples. The evolution of the temperature has
range in a homogeneous way on the whole outer surface. been simulated at the locations labelled 10 (top), 11 (middle)
Re-radiation with the environment is taken into account by and 12 (bottom), i.e., on the symmetry plane. Because of the
the simulation but the natural convection is not modelled. axisymmetry, the simulation does not distinguish the top and
the bottom side (near the injectors). Fig. 10 compares the
Since temperature is the key variable controlling the experiment (displayed in Fig. 6) and the simulation.
thermomechanical behavior of the tank and since the me- This comparison allows drawing the following conclusions:
chanical elastic stress does not influence the temperature
field, the Finite Element computation steps at each integration The model cannot correctly simulate the temperature close
point and each time increment are the following: to the outer surface. This is due to a large number of un-
certainties and hypotheses: fluctuation of the incident flux,
First a thermal analysis is run: the temperature is updated convection due to ambient air not taken into account, un-
by solving the heat equation. certainty about the exact location of the thermocouple in
Once the temperature is known, the mechanical properties the thickness (the “top” thermocouple is not directly stuck
(which depend on temperature) are modified. The rela- on the vessel surface but wound in the composite shell, in
tionship between temperature and stiffness is given in a the first outer layers)
tabular way, so that its evolution is in accordance with the The thermocouples in the composite wall (middle and
curves in Fig. 9. bottom) record much lower temperature than at the sur-
The mechanical stress components are updated and the face. This is due to the very low conductivity of the com-
local failure criterion is checked (the stress components posite material.
are compared to the mechanical strength at considered The model is capable of simulating accurately the tem-
temperature, details are given in the following). perature in the thickness.
Fig. 10 e Comparison experiment/simulation of the temperature evolution (incident flux 100 kW/m2).
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simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
12 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
computer time. When one of the following criteria is satisfied the outer layers redistributes the mechanical stress towards
at the ply scale: the inner layers and the vessel bursts when the remaining
s s s non-charred composite can no longer withstand the pressure.
11 22 12
ff ¼ 1 ¼ 0 ; fm ¼ 1 ¼ 0 ; fs ¼ 1 ¼ 0; (4) At lower inner pressures, the mechanical stress is not high
X Y S
enough to cause burst. Consequently, the liner has enough
failure initiates in the longitudinal, transverse or shear di- time to reach its melting temperature and the vessel leaks.
rection, respectively. The terms s11, s22 and s12 are respec- This section investigates the capability of the FE model
tively the in-plane longitudinal, transverse and shear stress detailed above to forecast this transition between burst and
components. The terms X, Y and S stand respectively for the leak regimes. Since the vessel may leak, a specific criterion
in-plane longitudinal, transverse and shear strengths. Due to detecting this phenomenon has to be considered. In a first
the tension stress state in the pressurized composite tank, approach, leak is assumed to occur as soon as the temperature
there is no need to distinguish tension and compression. The at the composite/liner interface reaches the liner polymer
aforementioned criteria are checked at each time increment melting point. Since the tightness in this type of structures is
and each integration point. When ff ¼ 0, fm ¼ 0 or fs ¼ 0 are only ensured by the liner (the composite porosity is about
satisfied, the local (at ply scale) longitudinal, transverse or 10%), liner melting is assumed to cause leak. In the following,
shear stiffness is set to 10% of its initial value. this melting temperature is taken equal to 135 C, according to
On the global (vessel) scale, the computations are found to [40].
diverge as soon as failure initiates in the longitudinal (fiber) di- The computation comprises two steps. In the first one, the
rection, i.e. as soon as ff ¼ 0, at an integration point of the inner pressure is applied (the initial pressure is chosen in the
structure. This first failure is found to occur in the cylindrical range 250 bare700 bar). In the second one, it is maintained
part. This rapid divergence can be explained by the fact that once constant and a flux of 100 kW/m2 is applied on the outer
fibers break in a composite layer, the stress is redistributed to the surface. As specified in the previous section, burst is detected
next layers, which will reach in turn very rapidly the ultimate when the fiber failure criterion ff ¼ 0 is reached in the cylinder.
stress level and then also break. This domino effect explains the In the following, the text refers to the “most loaded layer”, that
numerical divergence. This almost simultaneous occurrence of means the layer which undergoes the maximum stress in the
first fiber breakage at the ply scale and burst at the tank scale has fiber direction. This is the first layer that fulfils ff ¼ 0 and is the
already been highlighted in simulations of similar composite place of burst initiation. Fig. 11 plots:
tanks only subjected to an increasing inner pressure [21]: it is
shown that fibers start to break not before 98% of the burst (i) the evolution of ff (scale on the left-hand side of the
pressure, which is an evidence of a very rapid failure mecha- curve) in the most loaded layer. At each curve corre-
nism. This effect is even more marked in tanks subjected to fire: sponds a given value of the initial inner pressure
when the first fiber breakage occurs, 28% of the composite wall (ii) the evolution of the temperature in this most loaded
of the vessels studied here has reached or exceeds 350 C layer (solid red line, scale on the right-hand side)
(combustion onset temperature) and can be considered as a (iii) the evolution of the temperature at the interface com-
material with no mechanical strength. posite/liner in the cylinder (dashed red line, scale on the
Consequently in the following burst is assumed to occur as right-hand side)
soon as the criterion ff ¼ 0 is reached in any layer in the cyl-
inder. This criterion leads to the value of time to burst recor- According to the initial pressure value, different types of
ded in Table 1, for the vessel pressurized at 700 bar (the evolution can be observed for ff in the most loaded layer:
experimental results are displayed in Fig. 5):
The simple approach based on a fiber failure criterion At high inner pressure (f. ex. 700 bar):
provides a satisfactory time to burst. This validates the
strategy chosen here, i.e. the stiffness is controlled by tem- The value of ff rapidly increases. This is due to stress
perature, even when combustion occurs (the FE simulations redistribution when the temperature of the outer layers in-
do not refer to combustion reactions, combustion is taken into creases and their stiffness decreases. When ff crosses the
account through a stiffness drop when the ignition tempera- horizontal black solid line (ff ¼ 0.0), first fibers break and burst
ture is reached). occurs (at 228s for 700 bar).
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5 13
Fig. 11 e Evolution of the fiber failure criterion ff in the most loaded layer, of the temperature in this layer and of the
temperature at the interface liner-composite for an incident flux of 100 kW/m2.
this layer drops and so does ff. If the ff peak is above 0.0, the may leak if the melting point of the HDPE (135 C) is reached at
vessel may burst (for example at 430s for an inner pressure of the liner-composite interface before ff is equal to 0.0. This
400 bar). The limit configuration is for an inner pressure of transition occurs at 470s: if ff is less than 0.0 at 470s, the vessel
300 bar, when ff reaches 0.0 and starts to decrease. leaks. In the light of these considerations, it is possible to
draw, by the means of FE simulations at different inner
For low inner pressure (<300 bar): pressures, the safe pressure relief curve (Fig. 12) which con-
nects the critical (burst or leak) points and defines a safe zone
The ff curve does not cross (or even reach) the black solid (no burst/no leak). This curve is obtained in the following way:
line, the vessel cannot burst.
This analysis of the evolution of ff has to be associated to For a given inner pressure in the range 300 bare700 bar, the
the leak criterion. The transition from burst to leak is the evolution of ff is calculated. The time to burst corresponds
result of a competition between two different kinetics: the to the time at which ff reaches 0.0 (black dots in Fig. 12).
time needed for ff to reach 0.0 and the time needed by the If this dot is on the right side of the dashed line at 470s, the
liner-composite interface to reach 135 C. Indeed, the vessel temperature rise at the liner-composite interface is rapid
Please cite this article in press as: Halm D, et al., Composite pressure vessels for hydrogen storage in fire conditions: Fire tests and burst
simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088
14 i n t e r n a t i o n a l j o u r n a l o f h y d r o g e n e n e r g y x x x ( 2 0 1 7 ) 1 e1 5
enough to reach 135 C before burst, and the tank leaks to leak. The axisymmetric simulation provides reliable results
whatever the inner pressure. This transition occurs for an very quickly but is limited to engulfing fires. Since it gives a
initial inner pressure of about 370 bar. Therefore the safety good prediction of the burst and leak of the cylinders, it is a
curve is composed of two parts: firstly a decreasing curve useful tool to limit costly and complex test and to design
when the inner pressure is more than 370 bar and secondly pressure relief devices which may equip the hydrogen tanks
a vertical line at the point of abscissa 470s. to make sure the pressure always lies within the safe zone.
These results need of course to be confirmed by comple-
The comparison with experiments is fairly satisfactory, all mentary tests. In particular, the critical inner pressure range
the more since the incident flux cannot be accurately 350 bare450 bar should be further investigated. Note also that
measured during the fire tests and the value of 100 kW/m2 is the repeatability of the experimental data (often obtained
an upper bound. Moreover, only one vessel has been tested at from only one test) should be checked. The simulations
525 bar, 250 bar and 100 bar. Extra tests should be necessary to should also be extended to real 3D (and not only axisym-
confirm, or not, the repeatability. Fig. 12 gives rise to the metric) cases in order to deal with particular fire configura-
following comments: tions (localized impingement, non-homogeneous applied flux,
partly protected cylinders, …). Regarding modelling of the
The simulated times to burst at 700 bar and 525 bar are in material behavior, the burst criterion has to be improved: the
accordance with the experiment. use of a damage model capable of simulating the progressive
The simulation is capable of capturing the transition be- degradation of the composite and taking into account the
tween burst (above 370 bar) and leak (below). This pre- probabilistic nature of fiber breakage [41] is a way to better
dicted pressure is in accordance with the experimental simulate the burst pressure.
tests displayed in Fig. 7.
Considering the low number of tests in these conditions
(only two 36-L vessels have been tested below 370 bar) and
Acknowledgments
the simplicity of the leak criterion, the simulated time to
leak is quite satisfactory
The research leading to these results has received funding
from the European Union's Seventh Framework Program (FP7/
2007-2013) for the Fuel Cells and Hydrogen Joint Technology
Initiative under Grant Agreement No. 325329.
Concluding remarks The authors thank all partners for the amount of work
carried out in the FireComp project.
One of the objectives of the FireComp project was to generate
This work pertains to the French Government program
experimental data to understand the way pressurized com-
‘‘Investissements d’Avenir’’ (LABEX INTERACTIFS, reference
posite vessels behave when subjected to fire and to validate
ANR-11-LABX-0017-01).
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complete instrumentation of the tank was implemented to
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simulation, International Journal of Hydrogen Energy (2017), http://dx.doi.org/10.1016/j.ijhydene.2017.06.088